Process of producing titanium nitrogen compounds



FOORD VON BICHOWSKY .ANID'JOHN HARTHAN, 0F GLENDALE, CALIFORNIA.'

PROCESS OF PRODUCING TITANIUM NITROGEN COMPOUNDS.

No Drawing.

T 0 all whom it may concern: i I Be it known that we, FOORD VON BionowsxY and JOHN HARTHAN, citizens ofthe The present invention relates to a proo ess of producing titanium nitrogen and'the like compounds from such minerals as ilme-' nite and one off the important features'of the invention resides in the recovery or production of such compounds by heating ilmenite with an agent such as carbon and in the presence of an agent such as nitrogen. We have discovered that titanium oxide contained in such minerals as ilmenite ,(FeO.TiO or other titaniferous iron ores of the mineral; with an oxyg'encontaining salt of an alkali metal and carbon while passing nitrogen or impure mixtures of nitrogen, carbon. dioxide,'monoxide, methane and the like free from such other gases as sulphureted hydrogen which would harmfully cornbine with the constituents of the heated mass; at the temperatures slightly below that at which the'treated mass would melt.

The oxygen salt of the alkali metal may be either an oxide or hydroxideof sodium or potassium, or a carbonate. or formate or even a silicate or titanate of those metalsor mixtures of the above or any of their equivalents. be reduced and form harmful compounds such as iron' sulphide should not be em: ployed.

The carbon may be employed-for instance,

I in the form of soot, or coke, or of a com pound containing carbon, such for instance as crude oil, and instead of these, or in addition thereto, gases capable of yielding carbon, such as acetylene or methane or mixtures of the latter occurring as natural gas, may be passed over the heated mixture. By

this procedure the iron is reduced and saturated with carbon while the alkali. metal salt serves, together with the iron to catalytically accelerate the combination of the titanium with the nitrogen. From the mix-- Salts which like the sulphates would ture of iron and titanium nitride the iron is easily removed and the titanium nitride recovered. 7 j

A process based on the present invention is particularly valuable sincev the by-products, which may be obtained, have a wide commercial value and as a result the titanium nitridecanbe'obtained at a remark ably low figure. "Thus enabling use, to be made of it directly as an artificial fertilizer or it may be'employed as a source of pure titanium dioxide or other titanium salts.

Having now defined the purpose of our discovery the following examples will serve to illustrate further the nature of'our invention and the preferred method of carry ing it into practical effect, however it isnot confined to these examples as various de-.

partures may be found to bring about the desiredv result. The parts by weight are about as follows: v

100 parts ilmenite ground to pass 100 mesh, to the inch, screen, 5 parts anhydrous soda as :i '10 parts pitch, the whole worked and ma e into briquettes by-any suitable methodi These briquettes are then heated yfora period of about six hours during which t'ime-they are subjected to methane or nat-V ural gas under a slight pressure and con= taining about 20% by volume of nitrogen.

.At first, the temperature maybe between 11001200 C. but finally the temperature should be maintained between 1000-1100 C. to prevent the reduced iron, which by this time is saturated with carbon, from melt-' ing. Thetitanium nitride iron mixture so obtained is allowed to cool in an atmosphere of a neutral gas and when cold the iron'is dissolved out with warm dilute sulphuric acid. The ferrous sulphate solution, so obtained, is filtered and crystallized. The

titanium nitrides or cyanonitride or mixtures of both can be used for the preparation ofammonia or directly. as a fertilizer. As another example: I

parts ground ilmenite, 10 parts crude oil tar bri uetted and then heated in a stream parts water, the whole is well mixed and pressed into briquettes. Upon heating these of natura gas at about 1000 0., for three The improved process of thus producing sodium cyanide is not claimed as a part of the present invention but is divided and covered in a co-pending application. a 1

We claim: 1

1. The process of producing titanium nitrogen compounds which consists in heating ilmenite and oxygen salt, other than a thio acid of an alkali metal, in lesser quantity than would be required to convert all of the ilmenite into a titanate, with carbon in the presence of nitrogen.

2. The process of producing titanium nitrogen compounds which consists in heating ilmenite with carbon and sodium carbonate in the. resencej of nitrogen.

3. T e process of producing titanium nitrogen compounds which consists in heating ilmenite with carbon and sodium carbonate in the presence of nitrogen at'a temperature i to avoid fusing of the mass.

4. The process of producing titanium nitrogen compounds which consists in. heating ilmeiiite with carbon, sodium carbonate and nitrogen at a temperature of about 1100 C.

FOORD VON BIcHoWsKY. JOHN HARTHAN. 

